Available online at http://ijcpe.uobaghdad.edu.iq and www.iasj.net

Iraqi Journal of Chemical and Petroleum
Engineering

Vol.20 No.3 (September 2019) 31 – 37
EISSN: 2618-0707, PISSN: 1997-4884

Corresponding Authors: Name Huda M. Salman, Email: hudamohammad20@gmail.com , Name: Ahmed Abed Mohammed, Email:
ahmed.abedm@yahoo.com
IJCPE is licensed under a Creative Commons Attribution-NonCommercial 4.0 International License.

Removal of-Copper Ions-from Aqueous Solution Using Liquid-

Surfactant-Membrane Technique

Huda M. Salman

and Ahmed Abed Mohammed

Environmental Engineering Department, College of Engineering, University of Baghdad, Baghdad, Iraq

Abstract

Extraction of copper (Cu) from aqueous solution utilizing Liquid Membrane technology (LM) is more effective than precipitation

method that forms sludge and must be disposed of in landfills. In this work, we have formulated a liquid surfactant membrane (LSM)

that uses kerosene oil as the main diluent of LSM to remove copper ions from the aqueous waste solution through di- (2-ethylhexyl)

phosphoric acid - D2EHPA- as a carrier. This technique displays several advantages including one-stage extraction and stripping

process, simple operation, low energy requirement, and. In this study, the LSM process was used to transport Cu (II) ions from the

feed phase to the stripping phase, which was prepared, using H2SO4. For LSM process, various parameters have been studied such as

carrier concentration; treat ratio (TR), agitating speed and initial feed concentration. After finding the optimum parameters, it was

possible to extract Cu up to 95% from the aqueous feed phase in a single stage extraction.

Keywords: Copper, D2EHPA, Extraction, Surfactant, Liquid membrane

Received on 06/04/2019, Accepted on 28/05/2019, published on 30/09/1029

https://doi.org/10.31699/IJCPE.2019.3.5

1- Introduction

Increased use of metals and chemicals in process

industries has resulted in the generation of large quantities

of effluent that contain high levels of toxic heavy metals

and their presence poses disposal problems due to their

non-degradable and persistent nature. The most toxic

metals are aluminum, cobalt, chromium, iron, cadmium,

nickel, zinc, copper, lead and mercury, based on World

Health Organization (WHO) ‎[1]-‎[3]. The main industries

that add water pollution by chromium are leather tanning,

mining, electroplating, textile dyeing, coating operations,

aluminum conversion, and pigments. Removal of ions

from their effluents has assumed of a higher importance

in the recent past due to the decreasing availability of

natural resources and the increasing pollution in the

environment ‎[4]-‎[6].

The elimination of copper (Cu) from aqueous solutions

requires an efficient system for environmental reasons

(toxic ions when it above WHO limits). There is a general

concern to minimize the liquid effluents containing

dangerous metals. A traditional method to remove Cu

from solutions is the solvent extraction method. In this

technique, a well-established Cu extract should be used,

such as diketones or hydroxytoxics ‎[7].

LIX acid (Cognis) and di- (2-ethylhexyl) phosphoric

acid (D2EHPA), etc, the use of this carrier in the recovery

of Cu is well indicated elsewhere ‎[8]-‎[11].

Liquid Surfactant Membrane (LSM) has been

considered as an alternative to the solvent extraction for

separating solutes, like phenols, biochemical products,

and metal pollutants ‎[2], ‎[12]-‎[19].

LSM is a triple dispersion method, where a primary

emulsion (water/oil or oil/water) is dispersed in a feed

phase (E) to be treated. The liquid membrane comprises

from three phases i) internal ii) external, and iii) organic

phase. The organic phase contains a diluent, an emulsifier

to stabilize the emulsion, and an extractant in the case of

separation of metal ions ‎[10].

During the mixing between the feed phase (E) and

emulsion (organic + internal), the solute is transported

through the membrane into the stripping phase droplets

and is concentrated ‎[20].

After extraction, the emulsion is separated from the

raffinate phase and the demulsified of the emulsion is

usually performed by applying high voltage or heat. LSM

exhibit several advantages, such as re-extraction in a

single stage, large specific surface area for extraction,

simultaneous extraction, and the requirement of an

expensive extractant in small quantities ‎[10], ‎[21], ‎[22].

The objective of this work was to check the potential of

a liquid surfactant membrane, (LSM) for the extraction of

copper ions from the feed solution.

https://doi.org/10.31699/IJCPE.2019.3.5

H. M. Salman

and A. A. Mohammed / Iraqi Journal of Chemical and Petroleum Engineering 20,3 (2019) 31 - 37

Despite, studies in this field, the study investigate

various experimental parameters, like extractant

concentration, treatment ratio, agitation rate, and initial

feed concentration were examined, to identify the best

conditions, which would give the greatest performance of

the LSM.

2- Experimental Protocols

2.1. Reagents

The phosphorus acid di- (2-ethylhexyl) (D2EHPA)

functioned as a shuttle and Sorbitan monooleate (Span 80

C24H44O6) was the nonionic emulsifier, both reagents

were supplied by Sigma-Aldrich (Merck, Darmstadt,

Germany). Kerosene supplied by the Southern Oil

Company (SOC) (Al Basra-Iraq) used as a diluent, while

the sulphuric acid (H2SO4) was the eliminating agent and

was obtained from the factory producing acids and bases

(Babylon, Iraq). Copper solutions were prepared from

copper nitrate (Chemical, Company, Co., Ltd. Korea).

2.2. Procedure

The experimental work consists of four parts:

preparation of the emulsion as a first step, preparation of

stock solution, then running the extraction process and

finally the demulsification for emulsion. Fig. 1 illustrates

the procedure of LSM in this paper.

a. Emulsion preparation

Mixing certain volume of kerosene, Span80, and

D2EHPA at homogenizer (SR30 digital homogenizer,

model: 670/340 W, 10-2000ml, 3000-27000 rpm) speed

of 17500 rpm to get the oil phase. The sulphuric acid

(H2SO4) solution as a stripping agent was added dropwise

to the oil phase until the desired volume ratio of oil

solution to stripping solution was obtained. The solution

was stirred continuously for 10 min to obtain a stable

Water/Oil LSM.

b. Feed phase preparation

This phase was prepared by adding distilled water

(conductivity, 1μs/m) to Cu (NO3)2 (solid form) to get the

required concentrations (200 ppm) of copper and then

adding some drops of the sulphuric acid to reach pH equal

c. Extraction

All experiments were performed at a temperature of

25±1
°
C. The prepared emulsion (Error! Reference

source not found.) was added to a specific volume of

feed solution. The production of Water/Oil/Water double

emulsions was obtained from stirring the contents by a

digital stirrer (12700 rpm) for 12 min. Syringe and filter

syringe was used to draw external solution (E) and then

analyzed it by AAS (atomic absorption

spectrophotometry).

The resulted solution was allowed to separate to an

emulsion (Water/Oil) and an external solution (E) by

gravity in a separation funnel for 24 hours. After two-

phase separation, the external phase was drawn and the

concentration of Cu in the internal phase was analyzed

using AAS (Atomic Absorbtion Spectrophotometer). The

Cu(II) ions remain in membrane phase can be calculated

by mass balance. To know the significant variables

relating to the extraction of Cu, the extractant

concentration, initial Cu concentration, treat ratio (TR),

and stirring speed were varied to observe their effects on

Cu extraction.

d. Demulsification of the emulsion

After the extraction experiment, the loaded emulsion

was broken using a hot plate magnetic stirrer (70 °C for

43 min) into the internal Cu concentrated phase and the

organic phase. The internal phase (I) was analyzed and

after that determining Cu concentration.

Fig. 1. LSM technique,: (1) droplets, (2) organic phase,

(3) globules, (4) emulsifier and (5) internal phase and Cu

2.3. Extraction mechanism in the ELM system

The prepared emulsion (sec. ‎2.2 A) was transferred to

the external phase containing a certain concentration of

copper ions at pH 4 (adding some drops of 0.2 M

H2SO4).

A digital mixer was utilized to agitate the solution for

0–12 minutes. The extraction and stripping reactions of

the copper ions are elucidated in equation 1 and 2.

Where: RH refers to the protonated form of an

extracting (D2EHPA in this paper) ‎[23]. D2EHPA

structure is revealed in Fig. 2 ‎[24], ‎[25].

H. M. Salman

and A. A. Mohammed / Iraqi Journal of Chemical and Petroleum Engineering 20,3 (2019) 31 - 37

Fig. 2. Depicts the structure of D2EHPA

Extraction reaction of the copper ions:

   ( ) ( )
2 2 2 22S L

Cu RH PbR RH H   
(1)

Stripping reaction of the copper ions:

   ( ) ( )
22 2 2 22 S L

CuR RH H Cu RH   
(2)

Equation (1) denotes the reaction at the membrane (O) –

external (E) interface, while equation (2) shows the

reaction where the copper ions are stripped at the oil (O) –

internal (W) interface. The Cu (II) ions transfer by an

extracting from the external to the internal phase is

explained in Fig. 3. The extraction percentage (E%) is

found based on the equation (3) :

C - C

outinE% = ×100 %
C

in (3)

Where Cin is the initial copper concentration in the

external phase, and Cout is the copper ion concentration

post the extraction stage.

Fig. 3. Depicts the transfer mechanism of LSM

3- Results and Discussion

3.1. Effect of Changes in Carrier Concentration on

Copper Removal Efficiency

This paragraph presented in Fig. 4 as expected, as soon

as the mixing began, the first 0.5 min the extraction

efficiency increased due to the carrier's effectiveness in

carrying the copper ions as well as increasing the shuttle

D2EHPA concentration from 6% - 8% (v/v) provides only

2% increase in the quantity extracted using LSM.

At 10% D2EHPA, the % E slightly decreased. It should

be noted that under optimum conditions in the copper

extraction from nitrate solution it was observed that

D2EHPA concentration in the membrane phase in the

range of 2% (v/v) to 4% (v/v) decreased the rate of

extraction of copper as observed by ‎[2], ‎[23]. From an

economic point of view, an enhancement of 2% is very

low, so 6% D2EHPA is applied in the experiments.

Fig. 4. Effect of D2EHPA concentration on the Cu

extraction at optimal conditions, using LSM (O/I=1/1,

span 80=4 v/v%, H2SO4=0.5 M, feed concentration≈ 200

mg/L, pH=4, TR=1:10, mixing speed=250 rpm)

3.2. Effect of Changes of Stirring Speed on the Copper

Removal Efficiency

Another parameter affecting extraction to a large extent

was found to be stirring speed, and it has been studied in

the range 150 to 550 rpm using LSM1 and shown in Fig.

As the stirring speed increased from 150 to 250 rpm, the

removal of copper increased from 82% to 94.7% in 11

min time using LSM. This was due to the small size of the

globules (SSG) that were formed by shear force from the

impellers of the stirrer, which provided more interfacial

surface area for effective mass transfer. Above 11 min, no

copper was detected in the external phase due to

membrane breakage. However, as the stirring rate was

increased to 300 rpm, more shear was introduced into the

emulsion and external phase, which promotes emulsion

breakage.

For lower agitating speed, the interfacial contact area

and mass transfer between the external phase and

emulsion decreased due to the larger size of the emulsion.

A 250 rpm was suitable for satisfactory extraction

percentage. After 250-rpm extraction, percentage starts to

decline. Further increase in the mixing speed resulted in a

break of liquid surfactant membranes leading to an

outflow of extracted lead into the external phase.

This is because of a higher mixer speed which beyond

limits generally results in higher water transport into the

inner strip phase causing the membrane to

swell ‎[26], ‎[27]. Therefore, 250 rpm was chosen as the

optimum mixing speed for extraction of Cu (II).

H. M. Salman

and A. A. Mohammed / Iraqi Journal of Chemical and Petroleum Engineering 20,3 (2019) 31 - 37

Fig. 5. Effect, of stirring speed on a rate of copper

extraction using LSM

3.3. Effect of Changes of Treat Ratio (TR) on the Copper

Removal Efficiency

The treat ratio in an LSM extraction is the ratio of the

emulsion phase to feed phase. Increasing TR generally

leads to, an increase in the loading capacity, and the rate

of, extraction. This case happened due to existence

increment in emulsion volume and correspondingly an

increase in D2EHPA, and H2SO4 ‎[28], ‎[29].

Fig. 6 illustrates the effect of TR on the copper

extraction from copper nitrate solutions using LSM.

As TR increased there was an increase in the efficiency

of, this occurs when this ratio increased from 1:15 to 1:10.

This pattern could be recognized from a possible increase

in globule size distribution due to the increased hold-up of

the emulsion.

Sengupta et al. (2006) have noted a strong decline in the

extraction percentage of silver ions when TR was

increased from, 1:6 to 1:4 due to increased globule-size

distribution at larger emulsion hold-ups.

Fig. 6. Effect of (TR) on the Cu-extraction by LSM

The formation of LG (larger-globules) reduces the areas

of the outer surface and will increase the effective-length

of the diffusion pathways among the globule, causing a

low rate of Cu removal.

Treat ratios of 1:15, 1:10 and 1:5 indicate a considerable

increase in extraction capability at what time TR

increased from 1:15 to 1:10, due to, the increase in-

emulsion retention, the distribution of the size of globules

tended to change towards LG with a consequent reduction

in the rates.

3.4. Effect of Changes of Initial Copper Concentration on

Copper Removal Efficiency

The effect of initial Cu (II) ions concentrations in the

feed, on the rate of copper extraction, was investigated

using-emulsions having O/I=1/1, span80 =4 v/v % of the

organic phase and H2SO4=0.5 M, D2EHPA= 6% (v/v).

The initial (pH) and (TR) were kept at 4 and 1:10

respectively. Extraction results are displayed in Fig. 7 that

is a plot of the change in copper concentration in the feed

phase with time.

The pattern of copper loading in LSM along with a

quantitative assessment of the amount of copper stripped

in the internal-stripping phase of the emulsion, after a 12

min contact between the feed- and the LSM, for initial-

feed concentration variations, is presented in Fig. 8.

Fig. 7. Effect of initial-feed concentration on rate of

copper extraction using LSM (O/I=1/1, span 80 =,4 v/v%,

H2SO4=,0.5 M, D2EHPA=6%, feed concentration≈ 200

mg/L, pH=4, TR=1:10, mixing speed=250 rpm). (Cu IE,

initial-concentration of copper, in the external phase)

It was observed that as the initial-feed concentration

increased, the extent of copper-extraction-into LSM also

increased.-

When Cu loading was low most of the Cu extracted in

the membranes got stripped in the internal phase of the

membranes.

However, at high copper loadings, the amount of copper

stripped in the internal phase of the LSMs did not increase

substantially; hence most of the copper extracted by the

LSMs was retained in the membrane-phase‎[4], ‎[21], ‎[22].

H. M. Salman

and A. A. Mohammed / Iraqi Journal of Chemical and Petroleum Engineering 20,3 (2019) 31 - 37

Fig. 8. Copper extraction, stripping patterns in LSM (Int.,

internal phase; Roil, Retained in the oil phase; FExt, final

concentration in the external phase

The low percentage of Cu stripping could be recognized

from the slow stripping kinetics as well as the diffusional

effects that play an important role in further slowing

down the stripping rates. High values of CuIE (Initial

copper concentration) lead to greater copper loadings in

the LSMs causing, quick-saturation of the peripheral

internal-phase droplets in the emulsion necessitates

deeper-penetration of the Cu– D2EHPA complex within

the emulsion-globules to get stripped.

4- Conclusions

Extraction of copper Cu (II) from an aqueous phase was

studied utilizing a liquid surfactant membrane (LSM).

The membrane was composed of D2EHPA dissolved in

kerosene and span80 as a solvent as an emulsifier

respectively.

Sulfuric acid (H2SO4) was utilized as the stripping-

solution. The optimum conditions for Cu extraction are:

(a) 6-8% (v/v) D2EHPA concentration, (b) 4% (v/v)

span80 concentration, (c) 0.5 M H2SO4 concentration in

the internal-phase, (d) 1:1 the ratio of internal-phase to

membrane- phase, (e) acidity in external-phase is 4 ; (f)

external phase volume to membrane volume 1/10, (g)

extraction time, 11 minutes; and (h) agitating speed, 250

rpm.

The results also showed many parameters, stirring

speed, the D2EHPA concentration, feed concentration and

treating ratio, are very important in the extraction of Cu,

(2) the extraction efficiency (E) of Cu is 95% at 11 min.,

(3) at higher agitating speed of the water/oil/water

emulsion produces small emulsion droplets, consequently

increases the interface area of the carrier/Cu reaction.

However, it is necessary this paper considered a

maximum limit (250 rpm) to increase the extraction

efficiency, (4) the results showed that the LSM method is

a beneficial process to remove Cu from aqueous solution.

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H. M. Salman

and A. A. Mohammed / Iraqi Journal of Chemical and Petroleum Engineering 20,3 (2019) 31 - 37

إزالة أيونات النحاس من محلول مائي باستخدام تقنية الغشاء السطحي السائل

هدى محمد سلمان و احمد عبد محمد

العراق, بغدادقسم الهندسة البيئية, كمية الهندسة, جامعة بغداد,

الخالصة

أكثر فعالية من الطرق (LM) المحمول المائي باستخدام تقنية الغشاء السائلمن (Cu) يعد استخراج النحاس
التقميدية التي تنتج الحمأة ويجب ان يتم التخمص منها في مدافن النفايات. في هذا العمل ، قمنا بتكوين غشاء

حمول إلزالة أيونات النحاس من الممغشاء يستخدم زيت الكيروسين كمخفف رئيسي لـ (LSM) سطحي سائل
كناقل(. يعرض هذا – D2EHPA - ) (إيثيل هكسيل - 2المائية من خالل حامض الفسفوريك ثنائي اإليثيل )

األسموب العديد من المزايا مثل االنتقائية العالية، التشغيل البسيط، متطمبات الطاقة المنخفضة، عممية االستخراج
ة لنقل النحاس من مرحمة المحمول الخارجية إلى مرحمة والتجريد عمى مرحمة واحدة. وقد تم استخدام هذه الطريق

االنتزاع، التي تم إعدادها باستخدام حامض الكبريتيك، تمت دراسة العوامل المختمفة مثل تركيز الناقل ونسبة
وسرعة التحريك وتركيز النحاس األولي. بعد الحصول عمى العوامل المثمى، كان نسبة استخراج (TR) المعالجة
ممغم لكل لتر. 222٪ من المحمول المائي بتركيز اولي 59النحاس

.، استخراج، المثبت، الغشاء السائل : النحاس، الناقلالدالةكممات